反应 #1328403

ord-4e487b3cec564faea8c88468adbf93de

反应方程式

O=C1c2ccccc2-c2ccccc21
9-Fluorenone
NN.O
hydrazine monohydrate
Cl
hydrochloric acid
NN=C1c2ccccc2-c2ccccc21
9-fluorenone hydrazone
收率 74.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with a reflux condenser and a mechanical stirrer
  2. 2
    温度the mixture was refluxed for one hour
  3. 3
    过滤the crude solid product was harvested by filtration
  4. 4
    洗涤The solid was washed with isopropanol
  5. 5
    其他recrystallized from dioxane

实验过程

9-Fluorenone (200 g, 1.1 mol, from Aldrich, Milwaukee, Wis.) and hydrazine monohydrate (160 ml, 3.3 mol, from Aldrich, Milwaukee, Wis.) were dissolved in 1000 ml of 2-propanol in a 2000 ml 2-neck round bottom flask equipped with a reflux condenser and a mechanical stirrer. Concentrated hydrochloric acid (4 ml) was then added, and the mixture was refluxed for one hour. The mixture was cooled slowly to room temperature, and the crude solid product was harvested by filtration. The solid was washed with isopropanol and then recrystallized from dioxane to obtain 150 g (74% yield) of 9-fluorenone hydrazone.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07115347B2uspto-grants-2006_10